CN107346797A - Sapphire Substrate nano-pore preparation method - Google Patents
Sapphire Substrate nano-pore preparation method Download PDFInfo
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- CN107346797A CN107346797A CN201610296695.1A CN201610296695A CN107346797A CN 107346797 A CN107346797 A CN 107346797A CN 201610296695 A CN201610296695 A CN 201610296695A CN 107346797 A CN107346797 A CN 107346797A
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- sapphire substrate
- thin films
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- 239000000758 substrate Substances 0.000 title claims abstract description 54
- 229910052594 sapphire Inorganic materials 0.000 title claims abstract description 48
- 239000010980 sapphire Substances 0.000 title claims abstract description 48
- 239000011148 porous material Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000010409 thin film Substances 0.000 claims abstract description 43
- 229920002120 photoresistant polymer Polymers 0.000 claims abstract description 34
- 238000001312 dry etching Methods 0.000 claims abstract description 14
- 238000004528 spin coating Methods 0.000 claims abstract description 9
- 238000011161 development Methods 0.000 claims abstract description 4
- 238000012546 transfer Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 32
- 238000005530 etching Methods 0.000 claims description 26
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 9
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 8
- 230000008020 evaporation Effects 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 7
- 229910015844 BCl3 Inorganic materials 0.000 claims description 6
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000001020 plasma etching Methods 0.000 claims description 4
- 238000005260 corrosion Methods 0.000 claims description 3
- 230000007797 corrosion Effects 0.000 claims description 3
- 238000009616 inductively coupled plasma Methods 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 3
- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000000025 interference lithography Methods 0.000 abstract description 3
- 238000000605 extraction Methods 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 238000004026 adhesive bonding Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 238000001039 wet etching Methods 0.000 description 2
- -1 wherein Chemical compound 0.000 description 2
- XPDWGBQVDMORPB-UHFFFAOYSA-N Fluoroform Chemical compound FC(F)F XPDWGBQVDMORPB-UHFFFAOYSA-N 0.000 description 1
- 241001062009 Indigofera Species 0.000 description 1
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005566 electron beam evaporation Methods 0.000 description 1
- 239000010437 gem Substances 0.000 description 1
- 229910001751 gemstone Inorganic materials 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000000671 immersion lithography Methods 0.000 description 1
- 238000001459 lithography Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/005—Processes
- H01L33/0062—Processes for devices with an active region comprising only III-V compounds
- H01L33/0066—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound
- H01L33/007—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound comprising nitride compounds
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Weting (AREA)
Abstract
The present invention provides a kind of Sapphire Substrate nano-pore preparation method, comprises the following steps：One layer of monocrystal thin films are formed in sapphire substrate surface；One layer of photoresist of spin coating on the monocrystal thin films；Photoresist is exposed by litho machine；Development is carried out to the photoresist after exposure and forms nanometer hole pattern；Using the photoresist formed with nanometer hole pattern as monocrystal thin films described in mask dry etching, by the nano-pore pattern transfer to monocrystal thin films；Photoresist is removed, using the monocrystal thin films formed with the nanometer hole pattern as mask, dry etching is carried out to the Sapphire Substrate, by the nano-pore pattern transfer to the Sapphire Substrate；Remove the monocrystal thin films.Sapphire Substrate nano-pore preparation method proposed by the present invention, the nano-pore splicing block graphical sapphire substrate that dry etching technology Structures of Fast Realizing is uniform, the cycle is controllable, dutycycle is controllable, inexpensive is equipped with by laser interference lithography.
Description
Technical field
The present invention relates to semiconductor technical field of micro and nano fabrication, more particularly to a kind of Sapphire Substrate nano-pore system
Preparation Method.
Background technology
Because graphical substrate technology can not only reduce epitaxial gan layers dislocation density, raising crystal mass,
And the efficiency of light extraction of light emitting diode can be largely improved, therefore micron order graphical substrate technology exists
LED field is with extensive.At the same time the cycle of nano-patterned substrate structure is closely emitted wavelength, is also easy to produce
Bragg diffraction, and pattern density is big compared with micron order, therefore nano graph substrate efficiency of light extraction compares micron order
Graph substrate is more preferable.
Nano patterned method can be obtained at present mainly includes beamwriter lithography, liquid immersion lithography, nanometer
Impressing etc., these methods more or less can there is high processing costs, efficiency is low, repeatability is bad etc. lacks
Point.
The content of the invention
In order to solve the above problems, the present invention propose a kind of even structure, the cycle is controllable, dutycycle is controllable,
The Sapphire Substrate nano-pore preparation method of low cost.
Concrete technical scheme proposed by the present invention is：A kind of Sapphire Substrate nano-pore preparation method is provided, wrapped
Include following steps：
One layer of monocrystal thin films are formed in sapphire substrate surface；
One layer of photoresist of spin coating on the monocrystal thin films；
Photoresist is exposed, developed, to form a nanometer hole pattern；
Using the photoresist formed with nanometer hole pattern as monocrystal thin films described in mask dry etching, by the nanometer
Hole pattern is transferred on monocrystal thin films；
Photoresist is removed, using the monocrystal thin films formed with the nanometer hole pattern as mask, to the sapphire
Substrate carries out dry etching, by the nano-pore pattern transfer to the Sapphire Substrate；
Remove the monocrystal thin films.
Further, the monocrystal thin films are the silica monocrystal thin films that thickness is 200nm~300nm.
Further, the monocrystal thin films are formed by evaporation process in sapphire substrate surface, evaporation time
For 5~8 minutes.
Further, the photoresist is the positive photoresist that thickness is 200nm~300nm.
Further, the rotating speed of photoresist described in spin coating be 10000r/min, the time be 30 seconds, spin coating complete
Toasted 60 seconds at a temperature of 95 DEG C afterwards.
Further, the method for the exposure is interfered for three beam lasers.
Further, in the development step, developer solution is the sodium hydroxide solution that mass fraction is 8 ‰, is shown
The shadow time is 10~15 seconds.
Further, the dry etching monocrystal thin films use reactive ion etching process, etching gas SF6、
CHF3And He, wherein, SF6Flow is 5.5sccm, CHF3Flow is 32sccm, and He flows are 150sccm；
Radio-frequency power is 200W, and etch period is 2~4 minutes.
Further, the removal photoresist is using organic solvent ultrasonic cleaning method.
Further, the dry etching Sapphire Substrate uses inductively coupled plasma etching technique, carves
Erosion gas is Cl2And BCl3, wherein, Cl2Flow is 5~45sccm, BCl3Flow is 5~45sccm；Carve
Erosion power is 1000~3000W, and radio-frequency power is 100~500W, and sapphire substrate temperature is 20 DEG C, etching
1~3 minute time.
Further, the removal technique of the monocrystal thin films uses wet corrosion technique, the wet etching work
The etching liquid of skill is that volume proportion is 1:The mixed liquor of 5 hydrofluoric acid and ammonium fluoride, etching time are 10~120 seconds.
Sapphire Substrate nano-pore preparation method proposed by the present invention, by using three beam laser interference lithographies
Technique, it is only necessary to single exposure is carried out to photoresist, while monocrystal thin films are carried out using dry etch process
Etching, so as to which Structures of Fast Realizing is uniform, the cycle is controllable, dutycycle is controllable, the splicing of inexpensive nano-pore
Block graphics Sapphire Substrate, moreover, the nano-pore Sapphire Substrate that the present invention is formed can reduce epitaxial nitride
The dislocation density of thing, improve the efficiency of light extraction of light emitting diode.
Brief description of the drawings
The following description carried out in conjunction with the accompanying drawings, above and other aspect, the feature of embodiments of the invention
It will become clearer with advantage, in accompanying drawing：
Fig. 1 is Sapphire Substrate nano-pore preparation method flow chart；
Fig. 2-Fig. 7 is the structural representation of Sapphire Substrate nano-pore preparation process.
Embodiment
Hereinafter, with reference to the accompanying drawings to embodiments of the invention are described in detail.However, it is possible to many different
Form implements the present invention, and the present invention should not be construed as limited to the specific embodiment that illustrates here.
Conversely, there is provided these embodiments are in order to explain the principle and its practical application of the present invention, so that this area
Others skilled in the art it will be appreciated that various embodiments of the present invention and being suitable for the various of specific intended application and repairing
Change.
Reference picture 1, and with reference to shown in Fig. 2~Fig. 7, the present embodiment provides a kind of Sapphire Substrate nano-pore system
Preparation Method, it the described method comprises the following steps：
Step S1：One layer of monocrystal thin films 2 are deposited on the surface of Sapphire Substrate 1, the monocrystal thin films 2 are two
Silicon single crystal thin film is aoxidized, its thickness is 200nm~300nm, as shown in Figure 2；Wherein, monocrystal thin films 2 are logical
Cross the surface that evaporation process is formed at Sapphire Substrate 1, evaporation time is 5~8 minutes, and the specific time can be with
Depending on thicknesses of layers and evaporation environment, in other embodiments, monocrystal thin films can also use other
Material, for example, silicon nitride or carborundum, other works can also be used by forming the technique of the monocrystal thin films 2
Skill, for example, plasma enhanced vapor deposition, electron beam evaporation or magnetron sputtering etc..
Step S2：One layer of photoresist 3 of spin coating on monocrystal thin films 2, the photoresist 3 are positive photoresist,
Its thickness is 200nm~300nm；Wherein, the rotating speed of the glue spreader used in spin coating photoresist be 10000r/min,
The gluing time is 30 seconds, needs to toast 60 seconds formation photoresists 3 at a temperature of 95 DEG C after the completion of gluing, such as
Shown in Fig. 3.
Step S3：Photoresist 3 is exposed by stepper, wherein, exposure method is three light
Beam laser interference, using step-by-step scanning type photoetching technique, wherein, by square array of nanometer hole pattern, row are
Example, three light beams are respectively 80 microns of square light fields, and exposure area is the square of 2 feet of the length of side each time
Region, three light beams are projected and tiled to 2 feet of square area, the light field border meeting of each light beam respectively
There is 2 microns overlapping, so as to form 80 microns of exposure region of periodic arrangement on the surface of photoresist 3,
Nanometer hole pattern can also be other shapes in the present embodiment, not limit here.Three are used in the present embodiment
Beam laser interference only needs single exposure, relative to double light beam laser interference exposure frequency can subtract
Less once.
Step S4：Development is carried out to the photoresist 3 after exposure and forms photoresist nanometer hole pattern 31, such as Fig. 4
It is shown.Wherein, developer solution is the sodium hydroxide solution that mass fraction is 8 ‰, and developing time is 10~15 seconds,
The specific time is depending on exposure dose and exposition uniformity.
Step S5：It is mask with the photoresist 3 formed with nanometer hole pattern 31, is carved by dry etch process
Monocrystal thin films 2 are lost, nanometer hole pattern 31 is transferred on monocrystal thin films 2, obtained with nanometer hole pattern 21
Monocrystal thin films 2, as shown in Figure 5.Wherein, dry etching monocrystal thin films 2 are using reactive ion etching
Technique (RIE), it is SF to etch the gas used6、CHF3And He, SF6Flow is 5.5sccm, CHF3
Flow is 32sccm, and He flows are 150sccm；Radio-frequency power is 200W, and etch period is 2~4 minutes,
The specific time is according to the type of etching gas, the flow of etching gas, radio-frequency power and nanometer hole pattern
Shape determines.The present embodiment is performed etching using dry etch process to monocrystal thin films 2, relative to wet
For method etching technics, it is easier to control etch rate using dry etch process and etching homogeneity is more preferable.
Step S6：Photoresist 3 is removed, is mask with the monocrystal thin films 2 formed with nanometer hole pattern 21, it is right
Sapphire Substrate 1 carries out dry etching, and nanometer hole pattern 21 is transferred in Sapphire Substrate 1, obtains indigo plant
Jewel substrate nanometer hole pattern 11, as shown in Figure 6.Wherein, photoresist 3 is removed using organic solvent
Ultrasonic cleaning method, organic solution are acetone soln or isopropyl acetone solution；Dry etching Sapphire Substrate 1 is adopted
It is inductively coupled plasma (ICP) etching technics, etching gas Cl2And BCl3, wherein, Cl2
Flow is 5~45sccm, BCl3Flow is 5~45sccm；Etching power is 1000~3000W, radio frequency work(
Rate is 100~500W, and etching temperature is 20 DEG C, and etch period 1~3 minute, the specific time is according to etching gas
The type of body, the flow of etching gas, radio-frequency power, the shape of etching temperature and nanometer hole pattern are come true
It is fixed.
Step S7：Monocrystal thin films 2 are removed, as shown in Figure 7.Wherein, the buffer oxide that wet etching uses
Thing etching liquid (BOE) is the mixed liquor of hydrofluoric acid and ammonium fluoride, wherein, hydrofluoric acid and ammonium fluoride volume are matched somebody with somebody
Than for 1:5, etching time is 10~120 seconds, and the specific time is according to the proportioning and nanometer of BOE mixed liquors
The shape of hole pattern determines.
The Sapphire Substrate nano-pore preparation method that the present embodiment proposes, dry method is equipped with by laser interference lithography
The nano-pore splicing block that lithographic technique Structures of Fast Realizing is uniform, the cycle is controllable, dutycycle is controllable, inexpensive
Graphical sapphire substrate, the nano-pore Sapphire Substrate that the present invention is formed can reduce the dislocation of epitaxial nitride
Density, improve the efficiency of light extraction of light emitting diode.
Described above is only the embodiment of the application, it is noted that for the common of the art
For technical staff, on the premise of the application principle is not departed from, some improvements and modifications can also be made,
These improvements and modifications also should be regarded as the protection domain of the application.
Claims (11)
1. a kind of Sapphire Substrate nano-pore preparation method, it is characterised in that comprise the following steps：
One layer of monocrystal thin films are formed in sapphire substrate surface；
One layer of photoresist of spin coating on the monocrystal thin films；
Photoresist is exposed, developed, to form a nanometer hole pattern；
Using the photoresist formed with nanometer hole pattern as monocrystal thin films described in mask dry etching, by the nanometer
Hole pattern is transferred on monocrystal thin films；
Photoresist is removed, using the monocrystal thin films formed with the nanometer hole pattern as mask, to the sapphire
Substrate carries out dry etching, by the nano-pore pattern transfer to the Sapphire Substrate；
Remove the monocrystal thin films.
2. Sapphire Substrate nano-pore preparation method according to claim 1, it is characterised in that described
Monocrystal thin films are the silica monocrystal thin films that thickness is 200nm~300nm.
3. Sapphire Substrate nano-pore preparation method according to claim 2, it is characterised in that described
Monocrystal thin films are formed by evaporation process in sapphire substrate surface, and evaporation time is 5~8 minutes.
4. Sapphire Substrate nano-pore preparation method according to claim 1, it is characterised in that described
Photoresist is the positive photoresist that thickness is 200nm~300nm.
5. Sapphire Substrate nano-pore preparation method according to claim 4, it is characterised in that spin coating
The rotating speed of the photoresist is 10000r/min, the time is 30 seconds, is toasted after the completion of spin coating at a temperature of 95 DEG C
60 seconds.
6. Sapphire Substrate nano-pore preparation method according to claim 1, it is characterised in that described
The method of exposure is interfered for three beam lasers.
7. Sapphire Substrate nano-pore preparation method according to claim 1, it is characterised in that described
In development step, developer solution is the sodium hydroxide solution that mass fraction is 8 ‰, and developing time is 10~15 seconds.
8. Sapphire Substrate nano-pore preparation method according to claim 1, it is characterised in that described
Dry etching monocrystal thin films use reactive ion etching process, etching gas SF6、CHF3And He, wherein,
SF6Flow is 5.5sccm, CHF3Flow is 32sccm, and He flows are 150sccm；Radio-frequency power is
200W, etch period are 2~4 minutes.
9. Sapphire Substrate nano-pore preparation method according to claim 1, it is characterised in that described
Photoresist is removed using organic solvent ultrasonic cleaning method.
10. Sapphire Substrate nano-pore preparation method according to claim 1, it is characterised in that institute
State dry etching Sapphire Substrate and use inductively coupled plasma etching technique, etching gas Cl2With
BCl3, wherein, Cl2Flow is 5~45sccm, BCl3Flow is 5~45sccm；Etching power is
1000~3000W, radio-frequency power are 100~500W, and sapphire substrate temperature is 20 DEG C, etch period 1~3
Minute.
11. Sapphire Substrate nano-pore preparation method according to claim 1, it is characterised in that institute
The removal technique for stating monocrystal thin films uses wet corrosion technique, and the etching liquid of the wet corrosion technique is volume
Match as 1:The mixed liquor of 5 hydrofluoric acid and ammonium fluoride, etching time are 10~120 seconds.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610296695.1A CN107346797A (en) | 2016-05-06 | 2016-05-06 | Sapphire Substrate nano-pore preparation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610296695.1A CN107346797A (en) | 2016-05-06 | 2016-05-06 | Sapphire Substrate nano-pore preparation method |
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ID=60253162
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Cited By (3)
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| CN111439720A (en) * | 2020-03-13 | 2020-07-24 | 中国科学院物理研究所 | Method for preparing reducing nano structure |
| CN111675191A (en) * | 2020-06-03 | 2020-09-18 | 中国科学院物理研究所 | Method for producing three-dimensional nanostructures continuously adjustable in height |
| CN112635627A (en) * | 2019-10-08 | 2021-04-09 | 东莞市中图半导体科技有限公司 | Graphical composite substrate, preparation method thereof and LED epitaxial wafer |
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| CN111675191A (en) * | 2020-06-03 | 2020-09-18 | 中国科学院物理研究所 | Method for producing three-dimensional nanostructures continuously adjustable in height |
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Application publication date: 20171114 |
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| RJ01 | Rejection of invention patent application after publication |